Sodium Azide → 4-Chloro-3-cyanobenzyl azide

HRID 1194717노트

반응식

HRID 1194717 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6]Br)=[CH:4][C:3]=1[C:10]#[N:11].[N-:12]=[N+:13]=[N-:14].[Na+]>C(O)C>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][N:12]=[N+:13]=[N-:14])=[CH:4][C:3]=1[C:10]#[N:11]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 140330355-(Bromomethyl)-2-chlorobenzonitrile

생성물 1

HCID 230362384-Chloro-3-cyanobenzyl azide수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A stirred mixture of 4-chloro-3-cyanobenzyl bromide (3.0 g, 13 mmol) and sodium azide (1.26 g, 19.4 mmol) was refluxed 5 hours in absolute ethanol (30 mL). The mixture was kept 18 hours at ambient temperature, filtered, and the filtrate was evaporated under vacuum. The residue was triturated with diethyl ether, filtered, and evaporated to provide 2.45 g (98%) liquid 4-chloro-3-cyanobenzyl azide; I.R. (neat): 2240, 2100 cm1.

후처리

  1. filtrationfiltered
  2. customthe filtrate was evaporated under vacuum
  3. customThe residue was triturated with diethyl ether
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-2d9efaf094644f2fb1db6891b7fc2a98
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04816469

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